Zirconia dispersion, preparation method and use thereof

Abstract

To provide a zirconia dispersion, its preparation method, and its use.SOLUTION: The zirconia dispersion includes a zirconia ingredient, a dispersant, and a resin ingredient, and a zirconia material used as the zirconia ingredient has a D30 of 20nm or less, a D80 of 30nm or less, and a D95 of 100nm or less.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention is in the technical field of zirconia materials, and specifically relates to zirconia dispersions, their preparation methods and uses. [Background technology]

[0002] In recent years, transparent materials with high refractive index have been used in many fields, such as optical communication technology, optical computers, display panels, lenses, optical films, optical waveguides, solar cells and light-emitting diodes.

[0003] Optically transparent polymeric materials are widely used due to their advantages, such as low cost, good processability, and high visible light transmittance. However, most photocurable resins have relatively low refractive indices; for example, acrylate resins typically have a refractive index of 1.40 to 1.60. While the refractive index can be increased by changing the type and number of resin groups, such as by increasing the number of benzene ring structures, conjugated structures, and π electron structures in the molecule, if such structures are present in large quantities, the polymer will have light-scattering properties and a birefringence absorption coefficient, making it unsuitable as an optical material. For this reason, it is usually necessary to add a specific amount of inorganic nanoparticles to the photocurable resin to increase the refractive index of the photocurable resin.

[0004] Zirconia nanoparticles have advantages such as a high refractive index, high strength, high thermal stability, and chemical inertness. Dispersing inorganic zirconia nanoparticles in organic optical resins can significantly improve the optical performance of the organic resin and also improve the mechanical performance of the formed film. To ensure that such zirconia-resin dispersions can perform their functions in various optical fields, the dispersions must have not only high optical transmittance but also good rheological properties, which ensure continuity and stability in subsequent adhesive application processes (e.g., inkjet printing, spin coating, roll coating, etc.) and ensure the uniformity and functionality of the coated layer after curing. It is with this in mind that the present invention is provided. Summary of the Invention

[0005] The present invention aims to provide a zirconia dispersion, its preparation method and use, which solves or improves the above technical problems.

[0006] The present invention is realized as follows. In a first aspect, the present invention provides a zirconia dispersion, the zirconia dispersion comprising a zirconia component, a dispersant, and a resin component, The zirconia raw material used as the zirconia component is D 30 is 20 nm or less, and D 80 is 30 nm or less, and D 95 is 100 nm or less. In an alternative embodiment, the zirconia raw material used as the zirconia component is D 30 is 3nm to 20nm, and D 80 is 6nm to 30nm, and D 95 is 30nm to 100nm.

[0007] In an alternative embodiment, the zirconia raw material used as the zirconia component is D 30 is 3.87nm to 19.87nm, and D 80 is 6.46nm~29.55nm, and D 95 is 30.05nm to 95.05nm. In an alternative embodiment, the content of the zirconia raw material in the zirconia dispersion is 40 wt% to 75 wt%. In an alternative embodiment, the content of the zirconia raw material in the zirconia dispersion is 45 wt% to 70 wt%.

[0008] In an alternative embodiment, the content of the zirconia raw material in the zirconia dispersion is 50 wt% to 65 wt%. In an alternative embodiment, the zirconia component is obtained by modifying a zirconia raw material with a surface modifier. In an alternative embodiment, the amount of surface modifier used is 1 wt % to 30 wt % of the zirconia raw material.

[0009] In an alternative embodiment, the amount of surface modifier used is 5 wt% to 20 wt% of the zirconia raw material. In alternative embodiments, the surface modifier comprises at least one of an organic acid compound, a phosphonic acid compound, a coupling agent, and a chelating agent. In an alternative embodiment, the coupling agent is a silane coupling agent.

[0010] In an alternative embodiment, the amount of dispersant used is 1 wt% to 20 wt% of the zirconia raw material. In an alternative embodiment, the amount of dispersant used is 5 wt% to 10 wt% of the zirconia raw material. In an alternative embodiment, the resin component is an optical resin.

[0011] In an alternative embodiment, the resin component is a UV-curable acrylic resin. In an alternative embodiment, the zirconia dispersion comprises: Feature 1: 50s of zirconia dispersion -1 The viscosity value at the shear rate is less than 6000 mPa·s, Feature 2: 1000s of zirconia dispersions -1 The viscosity value at the shear rate is less than 4000 mPa·s. Feature 3: The rheology of the zirconia dispersion is 1.1 to 2.5, Feature 4: The transmittance of the zirconia dispersion liquid at a wavelength of 600 nm is 50% or more, Feature 5: The refractive index of the zirconia dispersion is greater than 1.65; The present invention has at least one of the characteristics 1 to 5.

[0012] In a second aspect, the present invention provides a method for preparing a zirconia dispersion according to any one of the above embodiments, comprising the steps of mixing a mixed solution containing an organic solvent, a zirconia component, and a dispersant with a resin component, and removing the organic solvent.

[0013] In an alternative embodiment, the content of the zirconia raw material in the mixed solution is 10 wt% to 80 wt%. In an alternative embodiment, the content of the zirconia raw material in the mixed solution is 20 wt% to 50 wt%. In an alternative embodiment, the content of the zirconia raw material in the mixed solution is 20 wt% to 30 wt%.

[0014] In an alternative embodiment, the organic solvent includes at least one of an alcohol, a ketone, an ether, an ester, an aliphatic hydrocarbon, an alicyclic hydrocarbon, and an aromatic solvent. In an alternative embodiment, the organic solvent comprises at least one of propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, toluene, methyl ethyl ketone, and butyl acetate.

[0015] In a third aspect, the present invention provides an optical path adjustment coating layer, wherein raw materials for preparing the optical path adjustment coating layer include a zirconia dispersion according to any one of the above embodiments. In an alternative embodiment, the raw materials for preparing the light path control coating layer further include an initiator. In an alternative embodiment, when the resin component is a UV-curable acrylic resin, the initiator is a photoinitiator.

[0016] In an alternative embodiment, the amount of initiator used is 1 wt % to 5 wt % of the zirconia dispersion. In an alternative embodiment, the method for preparing the light path adjustment coating layer includes the steps of applying a raw material for preparing the light path adjustment coating layer to the surface of a substrate and curing the raw material. In an alternative embodiment, the light transmittance of the substrate is 89% or greater.

[0017] In an alternative embodiment, the light transmittance of the substrate is 90% or greater. In alternative embodiments, the substrate comprises polyethylene terephthalate, triacetate cellulose, polycarbonate, or polymethyl methacrylate. In an alternative embodiment, a light path adjusting coating layer can be used to adjust the light path.

[0018] In alternative embodiments, the light path adjusting coating layer can be used in optical communication technology, optical computers, display panels, lenses, optical films, optical waveguides, solar cells, or light emitting diodes.

[0019] The present invention includes the following beneficial effects: The present invention relates to the D of zirconia nanoparticles in a zirconia dispersion system. 30 is 20nm or less and D 80 By making the D 30 nm or less, the particle size of the nanoparticles in the zirconia dispersion system is relatively uniform, and the particle size distribution of all nanoparticles is relatively narrow, thereby making it possible to obtain a zirconia dispersion with excellent rheological properties. 30 and D 80 When the zirconia nanoparticles satisfying the above range are used, when the zirconia dispersion system formed therefrom is cured to form a film, the nanoparticles are distributed relatively uniformly and densely, and the hardness of the coating layer after film formation can be improved. 30 and D 80 In addition, zirconia nanoparticles D 95 By specifying the above, the content of large particles in the entire zirconia dispersion can be effectively controlled, preventing the large particles from impairing the light transmission performance of the dispersion and contributing to improving the light transmission performance of the dispersion. The obtained zirconia dispersion has relatively good rheological properties and light transmission, and a relatively high refractive index. Furthermore, the light path control coating layer prepared using the zirconia dispersion has higher hardness, which can contribute to maintaining the stability and functionality of the product. DETAILED DESCRIPTION OF THE INVENTION

[0020] In order to clarify the objectives, technical solutions and advantages of the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely explained below. In the embodiments, specific conditions are not specified, but they can be carried out under conventional conditions or conditions recommended by the manufacturer. For reagents or equipment whose manufacturers are not specified, conventional products available on the market can be used.

[0021] The zirconia dispersion according to the present invention, its preparation method, and use will now be described in detail. The present invention provides a zirconia dispersion, which includes a zirconia component, a dispersant, and a resin component.

[0022] The zirconia raw material used as the zirconia component is D 30 is 20 nm or less, and D 80 is 30 nm or less, and D 95 The above zirconia raw material is of nano-order.

[0023] For example, the D of the zirconia raw material used as the zirconia component 30 is 20 nm, 18 nm, 16 nm, 14 nm, 12 nm, 10 nm, 8 nm, 6 nm, 4 nm, 2 nm, or 1 nm, or may be other values ​​in the range of 20 nm or less and greater than 0. 80 is 30 nm, 25 nm, 20 nm, 18 nm, 16 nm, 14 nm, 12 nm, 10 nm, 8 nm, 6 nm, 4 nm, 2 nm, or 1 nm, or may be other values ​​in the range of 30 nm or less and greater than 0. 95 may be 100 nm, 90 nm, 80 nm, 70 nm, 60 nm, 50 nm, 40 nm, 30 nm, 20 nm, or 10 nm, or other values ​​in the range less than or equal to 100 nm and greater than 0.

[0024] D 30 , D80 and D 95 When setting D 30 ≦20nm, D 80 ≦30nm, D 95 ≦100 nm must also be satisfied at the same time.

[0025] In some embodiments, the zirconia raw material used as the zirconia component is D 30 is 3nm to 20nm, and D 80 is 6 nm to 30 nm, and D 95 In some preferred embodiments, the zirconia raw material used as the zirconia component has a D 30 is 3.87nm to 19.87nm, and D 80 is 6.46nm~29.55nm, and D 95 is 30.05nm to 95.05nm.

[0026] As described above, the present invention provides a method for producing zirconia nanoparticles in a zirconia dispersion system. 30 is 20nm or less and D 80 By making the D 30 nm or less, the particle size of the nanoparticles in the zirconia dispersion system is relatively uniform, and the particle size distribution of all nanoparticles is relatively narrow, thereby making it possible to obtain a zirconia dispersion with excellent rheological properties. 30 and D 80 When the zirconia nanoparticles satisfying the above range are used, when the zirconia dispersion system formed therefrom is cured to form a film, the nanoparticles are distributed relatively uniformly and densely, and the hardness of the coating layer after film formation can be improved. 30 and D 80 In addition, zirconia nanoparticles D 95 By also specifying

[0045] above, the content of large particles in the entire zirconia dispersion can be effectively controlled, preventing the large particles from impairing the light transmission performance of the dispersion and contributing to improving the light transmission performance of the dispersion.

[0027] In the present invention, the crystal type of the zirconia raw material is not limited, and when used, zirconia raw material of a crystal type such as monoclinic, tetragonal or mixed crystal can be used.

[0028] In some embodiments, the content of the zirconia raw material in the zirconia dispersion is 40 wt% to 75 wt%, such as 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, or 75 wt%, or may be other values ​​within the range of 40 wt% to 75 wt%. In some preferred embodiments, the content of the zirconia raw material in the zirconia dispersion is 45 wt% to 70 wt%. In some more preferred embodiments, the content of the zirconia raw material in the zirconia dispersion is 50 wt% to 65 wt%.

[0029] If the content of the zirconia raw material in the zirconia dispersion is less than 45 wt%, the refractive index of the prepared dispersion is relatively low, which is unfavorable for adjusting the optical path, whereas if the content of the zirconia raw material in the zirconia dispersion is more than 75 wt%, the dispersion cannot be prepared.

[0030] As mentioned above, the D 30 , D 80 and D 95 A zirconia dispersion prepared by using zirconia raw materials that simultaneously satisfy the above ranges in the above-mentioned ratio of amounts used has relatively excellent rheological properties and relatively high light transmittance.

[0031] In some embodiments, the zirconia component is obtained by modifying a zirconia raw material with a surface modifier. By performing surface modification on the zirconia raw material, the surface properties of the zirconia raw material can be improved and groups that have an affinity for the resin can be grafted onto the surface. The method of surface modification is not limited, and examples thereof include polishing, heating, and mixing and stirring.

[0032] The type of surface modifier is not limited as long as it has affinity for the resin. In some embodiments, the surface modifier includes at least one of an organic acid compound having various groups, a phosphonic acid compound, a coupling agent, and a chelating agent.

[0033] In some preferred embodiments, the surface modifier is a silane coupling agent, for example, a silane containing a group such as an acrylate group, a (meth)acrylic group, an epoxy group, an alkyl group, an alkoxyl group, a vinyl group, a phenyl group, a methacryloxy group, an amino group, a chlorosilane group, a chloropropyl group, or a sulfhydryl group.

[0034] The amount of the surface modifier used is 1 wt% to 30 wt% of the zirconia raw material, such as 1 wt%, 5 wt%, 10 wt%, 15 wt%, 20 wt%, 25 wt%, or 30 wt%, or may be other values ​​within the range of 1 wt% to 30 wt%. In some preferred embodiments, the amount of the surface modifier used is 5 wt% to 20 wt% of the zirconia raw material.

[0035] In the present invention, the dispersant serves to assist dispersion and wetting. Commercially available dispersants and various types of dispersants can be used. Each dispersant can be used alone, or multiple dispersants can be used in combination. For example, the dispersant includes at least one of a polyether acid compound, a polyether amine compound, a polyether acid / amine mixture, an ester compound containing a phosphate group, and a polyether compound containing a phosphate group. The dispersion method can be, but is not limited to, ultrasonic waves, stirring, grinding, etc.

[0036] In some embodiments, the amount of dispersant used is 1 wt% to 20 wt% of the zirconia raw material, such as 1 wt%, 2 wt%, 5 wt%, 8 wt%, 10 wt%, 12 wt%, 15 wt%, 18 wt%, or 20 wt%, or other values ​​within the range of 1 wt% to 20 wt%. In some preferred embodiments, the amount of dispersant used is 5 wt% to 10 wt% of the zirconia raw material.

[0037] In the present invention, the resin component is an optical resin. In some preferred embodiments, the resin component is an ultraviolet-curable acrylic resin, and includes, for example and without limitation, at least one of benzyl acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl acrylate, phenyl methacrylate, biphenyl methacrylate, 4-nitrophenyl methacrylate, 4-nitrobenzyl methacrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, biphenylmethanol acrylate, 4-chlorophenyl methacrylate, orthophenylphenol ethyl acrylate, bisphenol diacrylate, hydroxyethyl acrylate, pentaerythritol tetraacrylate, and dipentaerythritol hexaacrylate.

[0038] In some embodiments, the amount of resin used can be obtained by subtracting the total content of the zirconia raw material, surface modifier, and dispersant in the zirconia dispersion from 100%.

[0039] In some embodiments, the zirconia dispersion is -1 The viscosity value at this shear rate is less than 6000 mPa·s, for example, 196 mPa·s to 5756 mPa·s.

[0040] In some embodiments, 1000s of the zirconia dispersion -1 The viscosity value at this shear rate is less than 4000 mPa·s, for example, 154 mPa·s to 3350 mPa·s.

[0041] In some embodiments, the rheology of the zirconia dispersion is between 1.1 and 2.5, for example, between 1.167 and 2.456.

[0042] In some embodiments, the transmittance of the zirconia dispersion at a wavelength of 600 nm is 50% or more, for example, 51.4% to 65.2%.

[0043] In some embodiments, the refractive index of the zirconia dispersion is greater than 1.65, preferably greater than 1.67, and more preferably greater than 1.70.

[0044] The present invention further provides a method for preparing the above-mentioned zirconia dispersion, which comprises the steps of mixing a mixed solution containing an organic solvent, a zirconia component, and a dispersant with a resin component, and then removing the organic solvent.

[0045] In some embodiments, first, a zirconia raw material is modified with a surface modifier to obtain a zirconia component, the zirconia component, a dispersant, and an organic solvent are mixed to obtain a mixed solution, the mixed solution is mixed with a resin component, and the organic solvent is removed to obtain a zirconia dispersion.

[0046] In some embodiments, the content of the zirconia raw material in the mixed solution is 10 wt% to 80 wt%, such as 10 wt%, 20 wt%, 30 wt%, 40 wt%, 50 wt%, 60 wt%, 70 wt%, or 80 wt%, or may be other values ​​within the range of 10 wt% to 80 wt%. In some preferred embodiments, the content of the zirconia raw material in the mixed solution is 20 wt% to 50 wt%. In some more preferred embodiments, the content of the zirconia raw material in the mixed solution is 20 wt% to 30 wt%.

[0047] In some embodiments, the amount of organic solvent used can be obtained by subtracting the total content of the zirconia raw material, the surface modifier, and the dispersant in the mixed solution from 100%.

[0048] In the present invention, the organic solvent is not specifically limited. In some embodiments, the organic solvent comprises at least one of alcohols, ketones, ethers, esters, aliphatic hydrocarbons, alicyclic hydrocarbons, and aromatics. In some preferred embodiments, the organic solvent comprises at least one of propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, toluene, methyl ethyl ketone, and butyl acetate.

[0049] In the present invention, the method for removing the organic solvent is not particularly limited, and for example and without limitation, the organic solvent can be removed by using a rotary evaporator or other vacuum rectification equipment.

[0050] The present invention further provides an optical path adjustment coating layer, wherein raw materials for preparing the optical path adjustment coating layer include the above-described zirconia dispersion. Furthermore, the raw materials for preparing the optical path adjusting coating layer further include an initiator. In an alternative embodiment, when the resin component is a UV-curable acrylic resin, the initiator is a photoinitiator.

[0051] The photoinitiator used in the present invention is not particularly limited. In some embodiments, the photoinitiator includes at least one cationic photoinitiator, such as a diazonium salt, a sulfonium salt, or an imidazole. In other embodiments, the photoinitiator includes at least one radical photoinitiator, such as a phosphorus-based, triazine-based, benzophenone-based, benzoin-based, oxime-based, acetone-based, aminoketone-based, ketone-based, anthraquinone-based, or aromatic phosphine oxide compound. In some preferred embodiments, the photoinitiator includes at least one of TPO, 1173, 184, and 907.

[0052] In some embodiments, the amount of photoinitiator used is between 1 wt% and 5 wt% of the zirconia dispersion, such as 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, or 5 wt%, or other values ​​within the range of 1 wt% to 5 wt%.

[0053] The present invention further provides a method for preparing the above-mentioned light path adjustment coating layer, which comprises the steps of applying a raw material for preparing the light path adjustment coating layer to the surface of a substrate and curing it.

[0054] The coating method is not particularly limited, and examples thereof include roll coating, spray coating, curtain coating, and spin coating. The substrate to be coated is not particularly limited, but is preferably a substrate with high transmittance. In some embodiments, the substrate has a light transmittance of 89% or more, preferably 90% or more. In some specific embodiments, the substrate includes polyethylene terephthalate, triacetate cellulose, polycarbonate, polymethyl methacrylate, or the like.

[0055] Curing methods can be achieved by methods such as, for example and without limitation, mercury lamps and LEDs. The optical path adjustment coating layer has a relatively high hardness. The present invention also provides a use of the above-mentioned light path adjusting coating layer, which can be used to adjust the light path.

[0056] In some embodiments, the light path adjusting coating layer can be used in optical communication technology, optical computers, display panels, lenses, optical films, optical waveguides, solar cells, or light emitting diodes. Optical films include anti-reflection films.

[0057] The features and performance of the present invention will be described in more detail below with reference to examples. Example 1 The present invention provides a light path adjustment coating layer, and a method for preparing the light path adjustment coating layer includes the following steps: Step 1: 51 g zirconia raw material powder (D) with 5.1 g 3-(methacryloyloxy)propyltrimethoxysilane as the silane coupling agent 30 :16.85nm, D 80 :21.98nm, D 95 Modified zirconia was obtained by modifying the zirconia (particle size: 37.82 nm). The modified zirconia was dispersed in an organic solvent, propylene glycol monomethyl ether, by ball milling using 2.55 g of BYK-111 as a dispersant to obtain a mixed solution. The content of the zirconia raw material powder in the mixed solution was 30 wt%. Step 2: 41.35 g of 3-phenoxybenzyl acrylate was taken as a resin component and added to the above mixed solution, and the propylene glycol monomethyl ether was removed using a rotary evaporator to obtain a zirconia dispersion with a refractive index RI of more than 1.65. Step 3: 2 wt % of TPO, a photoinitiator, was added to the above zirconia dispersion, and the mixture was applied to PET and photocured to form a film, thereby obtaining an optical path adjusting coating layer.

[0058] Example 2 The present invention provides a light path adjustment coating layer, and a method for preparing the light path adjustment coating layer includes the following steps: Step 1: 58 g of zirconia raw material powder (D) was mixed with 5.8 g of 3-(methacryloyloxy)propyltrimethoxysilane as a silane coupling agent. 30 :9.53nm, D 80 :15.28nm, D 95 Modified zirconia was obtained by modifying the zirconia (particle size: 34.71 nm). The modified zirconia was dispersed in an organic solvent, propylene glycol monomethyl ether, by ball milling using 2.9 g of BYK-111 as a dispersant to obtain a mixed solution. The content of the zirconia raw material powder in the mixed solution was 30 wt%. Step 2: 33.3 g of 3-phenoxybenzyl acrylate was taken as a resin component and added to the above mixed solution, and the propylene glycol monomethyl ether was removed using a rotary evaporator to obtain a zirconia dispersion with a refractive index RI of more than 1.67. Step 3: 2 wt % of TPO, a photoinitiator, was added to the above zirconia dispersion, and the mixture was applied to PET and photocured to form a film, thereby obtaining an optical path adjusting coating layer.

[0059] Example 3 The present invention provides a light path adjustment coating layer, and a method for preparing the light path adjustment coating layer includes the following steps: Step 1: 62 g of zirconia raw material powder (D) was mixed with 6.2 g of 3-(methacryloyloxy)propyltrimethoxysilane as a silane coupling agent. 30 :19.54nm, D 80 :28.98nm, D 95 Modified zirconia was obtained by modifying the zirconia (39.22 nm). The modified zirconia was dispersed in an organic solvent, propylene glycol monomethyl ether, by ball milling using 3.1 g of BYK-111 as a dispersant to obtain a mixed solution. The content of the zirconia raw material powder in the mixed solution was 30 wt%. Step 2: 28.7 g of 3-phenoxybenzyl acrylate was taken as a resin component and added to the above mixed solution, and the propylene glycol monomethyl ether was removed using a rotary evaporator to obtain a zirconia dispersion with a refractive index RI of more than 1.70. Step 3: 2 wt % of TPO, a photoinitiator, was added to the above zirconia dispersion, and the mixture was applied to PET and photocured to form a film, thereby obtaining an optical path adjusting coating layer.

[0060] Example 4 This example differs from Example 1 in the following points: The zirconia raw material powder is D 30 is 13.48 nm, and D 80 is 17.20 nm, and D 95 The particle size was 35.51 nm and the dispersant was BYK-180. The refractive index RI of the zirconia dispersion according to this example was greater than 1.65.

[0061] Example 5 This example differs from Example 2 in the following points: The zirconia raw material powder is D 30 is 7.63 nm, and D 80 is 10.28 nm, and D 95 The particle size was 33.46 nm and the dispersant was BYK-180. The refractive index RI of the zirconia dispersion according to this example was greater than 1.67.

[0062] Example 6 This example differs from Example 3 in the following points: The zirconia raw material powder is D 30 is 3.87 nm, and D 80 is 6.46 nm, and D 95 The particle size was 30.05 nm and the dispersant was BYK-180. The refractive index RI of the zirconia dispersion according to this example was greater than 1.70.

[0063] Example 7 This example differs from Example 1 in the following points: The zirconia raw material powder is D 30 is 17.45 nm, and D 80 is 27.58 nm, and D 95 The particle diameter was 38.36 nm, the silane coupling agent was trimethyl[(2-methylallyl)oxy]silane (CAS number: 25195-85-1), and the dispersant was BYK-9010. The refractive index RI of the zirconia dispersion according to this example was greater than 1.65.

[0064] Example 8 This example differs from Example 2 in the following points: The zirconia raw material powder is D 30 is 18.37 nm, and D 80 is 29.55 nm, and D 95was 95.05 nm, the silane coupling agent was trimethyl[(2-methylallyl)oxy]silane, and the dispersant was BYK-9010. The refractive index RI of the zirconia dispersion according to this example was greater than 1.67.

[0065] Example 9 This example differs from Example 3 in the following points: The zirconia raw material powder is D 30 is 19.87 nm, and D 80 is 28.46 nm, and D 95 The particle size was 80.39 nm, the silane coupling agent was trimethyl[(2-methylallyl)oxy]silane, and the dispersant was BYK-9010. The refractive index RI of the zirconia dispersion according to this example was greater than 1.70.

[0066] Comparative Example 1 This comparative example differs from Example 1 in the following points: 30 is 22.77 nm, and D 80 is 33.96 nm, and D 95 was 108.25 nm.

[0067] Comparative Example 2 This comparative example differs from Example 2 in the following points: 30 is 22.77 nm, and D 80 is 33.96 nm, and D 95 was 112.52 nm.

[0068] Comparative Example 3 This comparative example differs from Example 3 in the following respects: The zirconia raw material powder was D 30 is 22.77 nm, and D 80 is 33.96 nm, and D 95 was 123.56 nm.

[0069] Comparative Example 4 This comparative example differs from Example 4 in the following respects: The zirconia raw material powder was D 30 is 28.32 nm, and D 80 is 37.13m, and D 95 was 128.46 nm.

[0070] Comparative Example 5 This comparative example differs from Example 5 in the following respects: The zirconia raw material powder was D 30 is 28.32 nm, and D 80 is 37.13 nm, and D 95 was 135.46 nm.

[0071] Comparative Example 6 This comparative example differs from Example 6 in the following respects: The zirconia raw material powder was D 30 is 28.32 nm, and D 80 is 37.13 nm, and D 95 was 141.46 nm.

[0072] Comparative Example 7 This comparative example differs from Example 7 in the following respects: The zirconia raw material powder was D 30 is 32.92 nm, and D 80 is 40.56 nm, and D 95 was 146.23 nm.

[0073] Comparative Example 8 This comparative example differs from Example 8 in the following respects: The zirconia raw material powder was D 30 is 32.92 nm, and D 80 is 40.56 nm, and D 95 was 147.23 nm.

[0074] Comparative Example 9 This comparative example differs from Example 9 in the following respects: The zirconia raw material powder was D 30 is 32.92 nm, and D 80 is 40.56 nm, and D 95 was 156.23 nm.

[0075] Comparative Example 10 This comparative example differs from Example 1 in the following points: 30 is 18.11 nm, and D 80 is 32.54 nm, and D 95 was 108.29 nm.

[0076] Comparative Example 11 This comparative example differs from Example 1 in the following points: 30 is 23.62 nm, and D 80 is 28.74 nm, and D 95 was 105.36 nm.

[0077] Comparative Example 12 This comparative example differs from Example 1 in the following points: 30 is 27.52 nm, and D 80 is 36.88 nm, and D 95 was 96.49 nm.

[0078] Comparative Example 13 This comparative example differs from Example 1 in the following points: 30 is 17.44 nm, and D 80 is 27.62 nm, and D 95 was 107.41 nm.

[0079] Comparative Example 14 This comparative example differs from Example 1 in the following points: 30 is 18.36 nm, and D 80 is 32.59 nm, and D 95 was 93.72 nm.

[0080] Comparative Example 15 This comparative example differs from Example 1 in the following points: 30 is 22.92 nm, and D 80is 28.98 nm, and D 95 was 96.66 nm.

[0081] Comparative Example 16 This comparative example differs from Example 1 in the following respects: The zirconia raw material powder had a pore volume of 0.0372 cm 3 / g, pore size is 0.8645 nm, average particle size is 10 nm, D 30 is 18.22 nm, and D 80 is 36.54 nm, and D 95 was 110.32 nm.

[0082] Test Example <1> The zirconia dispersions prepared in Examples 1 to 9 and Comparative Examples 1 to 16 were subjected to the following tests. A. Shear rate is 50 s -1 The viscosity value was measured under the conditions and its unit was mPa·s. B. Shear rate is 1000 s -1 The viscosity value was measured under the conditions and its unit was mPa·s. C. Measure the rheology. Rheology value = shear rate 50 s -1 Viscosity measured under the condition of shear rate of 1000 s -1 The viscosity values ​​were measured under the following conditions. D. The light transmittance was measured under the condition that the wavelength was 600 nm, and the unit was %.

[0083] <2> The optical path adjusting coating layers prepared in each of Examples 1 to 9 and Comparative Examples 1 to 16 were subjected to a hardness test in accordance with "GBT6739-1996 Pencil Hardness Measurement Method for Coated Films."

[0084] The test results are shown in Tables 1 to 3.

[0085] [Table 1]

[0086] [Table 2]

[0087] [Table 3]

[0088] As can be seen from Tables 1 to 3, the zirconia dispersions prepared in Examples 1 to 9 had better rheological properties and light transmittance, and relatively higher refractive indices, than the zirconia dispersions prepared in Comparative Examples 1 to 16. Furthermore, the optical path adjusting coating layers prepared in Examples 1 to 9 had higher hardness than the optical path adjusting coating layers prepared in Comparative Examples 1 to 16, which can contribute to maintaining the stability and functionality of the product.

[0089] As described above, the present invention provides a method for producing zirconia nanoparticles in a zirconia dispersion system. 30 is 20nm or less and D 80 By making the D 30 nm or less, the particle size of the nanoparticles in the zirconia dispersion system is relatively uniform, and the particle size distribution of all nanoparticles is relatively narrow, thereby making it possible to obtain a zirconia dispersion with excellent rheological properties. 30 and D 80 When the zirconia nanoparticles satisfy the above range, the nanoparticles are distributed relatively uniformly when the zirconia dispersion liquid system formed therefrom is cured to form a film, and the hardness of the coating layer after film formation can be improved. 30 and D 80 In addition, zirconia nanoparticles D 95 By specifying the above, the content of large particles in the entire zirconia dispersion can be effectively controlled, preventing the large particles from impairing the light transmission performance of the dispersion and contributing to improving the light transmission performance of the dispersion. The obtained zirconia dispersion has relatively good rheological properties and light transmission, and a relatively high refractive index. Furthermore, the optical path control coating layer prepared using the zirconia dispersion has higher hardness, which contributes to maintaining the stability and functionality of the product.

[0090] The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. Those skilled in the art will appreciate that the present invention may have various modifications and variations. Any modifications, equivalent replacements, improvements, etc. made without departing from the spirit and principle of the present invention are within the scope of protection of the present invention.

Claims

1. A zirconia dispersion comprising: Contains a zirconia component, a dispersant, and a resin component, The zirconia raw material used as the zirconia component is D ３０ is 20 nm or less, and D ８０ is 30 nm or less, and D ９５ is 100 nm or less A zirconia dispersion characterized by:

2. The zirconia raw material used as the zirconia component is D ３０ is 3 nm to 20 nm, and D ８０ is 6 nm to 30 nm, and D ９５ is 30 nm to 100 nm The zirconia dispersion according to claim 1 .

3. The content of the zirconia raw material in the zirconia dispersion is 40 wt % to 75 wt %. The zirconia dispersion according to claim 1 .

4. The zirconia component is obtained by modifying the zirconia raw material with a surface modifier, Preferably, the amount of the surface modifier used is 1 wt % to 30 wt % of the zirconia raw material, Preferably, the surface modifier includes at least one of an organic acid compound, a phosphonic acid compound, a coupling agent, and a chelating agent. The zirconia dispersion according to claim 1 .

5. The amount of the dispersant used is 1 wt % to 20 wt % of the zirconia raw material, Alternatively, the resin component is an optical resin. The zirconia dispersion according to claim 1 .

6. Feature 1: The zirconia dispersion －１ The viscosity value at a shear rate of is less than 6000 mPa s; Feature 2: 1000s of the zirconia dispersion －１ The viscosity value at a shear rate of is less than 4000 mPa s; Feature 3: The rheology of the zirconia dispersion is 1.1 to 2.5; Feature 4: the transmittance of the zirconia dispersion at a wavelength of 600 nm is 50% or more; Feature 5: The refractive index of the zirconia dispersion is greater than 1.65; The present invention has at least one of the characteristics 1 to 5. The zirconia dispersion according to claim 1 .

7. A method for preparing the zirconia dispersion according to any one of claims 1 to 6, comprising: a step of mixing a mixed solution containing an organic solvent, a zirconia component, and a dispersant with a resin component, and removing the organic solvent; Preferably, the content of the zirconia raw material in the mixed solution is 10 wt % to 80 wt %, Preferably, the organic solvent includes at least one of an alcohol, a ketone, an ether, an ester, an aliphatic hydrocarbon, an alicyclic hydrocarbon, and an aromatic solvent. A method for preparing a zirconia dispersion, comprising:

8. An optical path adjusting coating layer, A raw material for preparing the optical path adjusting coating layer contains the zirconia dispersion according to any one of claims 1 to 6, Preferably, the raw materials for preparing the optical path adjusting coating layer further include an initiator, Preferably, the amount of the initiator used is 1 wt % to 5 wt % of the zirconia dispersion; Preferably, the hardness of the optical path adjusting coating layer is 2B. An optical path adjusting coating layer characterized by:

9. 9. A method for preparing an optical path adjusting coating layer according to claim 8, comprising: A step of applying a raw material for preparing the optical path adjustment coating layer to a surface of a substrate and curing the raw material; Preferably, the light transmittance of the substrate is 89% or more, Preferably, the substrate comprises polyethylene terephthalate, triacetate cellulose, polycarbonate, or polymethyl methacrylate.

1. A method for preparing an optical path adjusting coating layer, comprising:

10. Use of the optical path adjustment coating layer according to claim 8, The optical path adjusting coating layer can be used to adjust the optical path, Preferably, the optical path adjusting coating layer can be used in optical communication technology, optical computers, display panels, lenses, optical films, optical waveguides, solar cells or light emitting diodes.

1. Use of a light path adjusting coating layer.

Images